DIN ISO 8454-2012 Cigarettes - Determination of carbon monoxide in the vapour phase of cigarette smoke - NDIR method (ISO 8454 2007 + Amd 1 2009)《卷烟 烟雾气相中一氧化碳含量测定 非色散红外分析法》.pdf

1、February 2012 Translation by DIN-Sprachendienst.English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC

2、S 65.160!$ys“1868057www.din.deDDIN ISO 8454Cigarettes Determination of carbon monoxide in the vapour phase of cigarettesmoke NDIR method (ISO 8454:2007 + Amd.1:2009)English translation of DIN ISO 8454:2012-02Zigaretten Bestimmung des Kohlenmonoxidgehalts in der Gasphase von Zigarettenrauch NDIR-Verf

3、ahren (ISO 8454:2007 + Amd.1:2009)Englische bersetzung von DIN ISO 8454:2012-02Cigarettes Dosage du monoxyde de carbone dans la phase gazeuse de fume de cigarette Mthode IRND (ISO 8454:2007 + Amd.1:2009)Traduction anglaise de DIN ISO 8454:2012-02SupersedesDIN ISO 8454:2009-08www.beuth.deDocument com

4、prises pagesIn case of doubt, the German-language original shall be considered authoritative.1102.12 A comma is used as the decimal marker. Contents Page National foreword .3 National Annex NA (informative) Bibliography .3 2 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions5

5、 4 Principle 5 5 Apparatus .5 6 Standard gas mixtures 6 7 Procedure .6 8 Expression of results 8 9 Repeatability and reproducibility .8 10 Test report 9 Bibliography 11 DIN ISO 8454:2012-02 DIN ISO 8454:2012-02 3 National foreword This standard has been prepared by Technical Committee ISO/TC 126 “To

6、bacco and tobacco products” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Products Standards Committee), Working Committee NA 057-04-01 AA Tabak und Tabakerzeugnisse. T

7、he text of ISO 8454:2007 + Amd. 1:2009 has been adopted in this standard without any modification. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. DIN shall not be held responsible for identifying any or all such patent rights. Th

8、e start and finish of text introduced or altered by amendment is indicated in the text by a vertical line in the left margin. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3308 DIN ISO 3308 ISO 3402 DIN ISO 3402 ISO 4387 DIN ISO 4387

9、ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DIN ISO 8454:2009-08 as follows: a) an Introduction has been included (ISO 8454:2007/Amd. 1:2009) stating that no machine smoking regime can represent all human smoking behaviour. The technical substance of the

10、 standard has not been changed. Previous editions DIN 10248: 1990-07 DIN ISO 8454: 1997-03, 2009-08 National Annex NA (informative) Bibliography DIN ISO 3308, Routine analytical cigarette-smoking machine Definitions and standard conditions DIN ISO 3402, Tobacco and tobacco products Atmosphere for co

11、nditioning and testing DIN ISO 4387, Cigarettes Determination of total and nicotine-free dry particulate matter using a routine analytical smoking machine DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, A

12、ccuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method Introduction No machine smoking regime can represent all human smoking behaviour: it is recommended that cigarettes als

13、o be tested under conditions of a different intensity of machine smoking than those specified in this International Standard; machine smoking testing is useful to characterize cigarette emissions for design and regulatory purposes, but communication of machine measurements to smokers can result in m

14、isunderstandings about differences in exposure and risk across brands; smoke emission data from machine measurements may be used as inputs for product hazard assessment, but they are not intended to be nor are they valid as measures of human exposure or risks. Communicating differences between produ

15、cts in machine measurements as differences in exposure or risk is a misuse of testing using ISO standards. Cigarettes Determination of carbon monoxide in the vapour phase of cigarette smoke NDIR method4 DIN ISO 8454:2012-02 1ScopeThis International Standard specifies a method for the determination o

16、f carbon monoxide (CO) in the vapourphase of cigarette smoke.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For datedreferences, only the edition cited applies. For undated references, the latest edition of the referenced document(inc

17、luding any amendments) applies.ISO 3308, Routine analytical cigarette-smoking machine Definitions and standard conditionsISO 3402, Tobacco and tobacco products Atmosphere for conditioning and testingISO 4387, Cigarettes Determination of total and nicotine-free dry particulate matter using a routine

18、analyticalsmoking machine3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1 vapour phaseportion of smoke, which passes the particulate phase trap during smoking in accordance with ISO 4387 using amachine conforming to ISO 33083.2 clearing puffany

19、puff taken after a cigarette has been extinguished or removed from the cigarette holder4 PrincipleSmoking of cigarettes in accordance with the procedures given in ISO 4387. Collection of the vapour phase ofthe cigarette smoke and measurement of the carbon monoxide using a non-dispersive infrared (ND

20、IR) analysercalibrated for carbon monoxide. Calculation of the amount of carbon monoxide per cigarette.5 ApparatusUsual laboratory apparatus and, in particular, the following items.5.1 Conditioning enclosure, maintained accurately in accordance with the conditions specified in ISO 3402,for condition

21、ing the cigarette sample prior to smoking (see also 7.1).5.2 Routine analytical cigarette-smoking machine and accessories, complying with the requirements ofISO 3308.5 DIN ISO 8454:2012-02 5.3 Vapour-phase collection system, which can be fitted to one or more of the smoking machine channels.The use

22、of the system shall ensure collection of all the vapour phase (normally vented to atmosphere) to bestored in a previously evacuated container for subsequent sampling through an NDIR analyser.The collection system shall not cause interference with the normal performance of the smoking machine andthe

23、consequent determination of total particulate matter and nicotine.The impermeability of the gas-collecting device to a vapour phase shall be checked with a vapour phasecontaining a volume fraction of to of CO. The CO concentration shall be measured directly after fillingthe previously evacuated gas-

24、collecting device. After a period of not less than , the measured value of COconcentration in the vapour phase in the device shall not differ by more than a volume fraction of from thevalue expected from the first determination.When a bag is used as the gas-collecting device, it shall be large enoug

25、h to avoid the final pressure of itscontents exceeding the ambient atmospheric pressure. The volume of the bag should also be no greater thantwice the volume of the gas content collected at atmospheric pressure. In practice, the collection of the vapourphase from 5 cigarettes requires a volume of an

26、d the collection of the vapour phase from 20 cigarettesrequires a volume of .5.4 Non-dispersive infrared (NDIR) analyser, selective and calibrated for the measurement of carbonmonoxide in vapours and gases.Analysers are available from several manufacturers and should have a preferred working range o

27、f a volumefraction of to CO and a sampling rate of between and . The analyser shall have aprecision of of full scale, a linearity of of full scale and a repeatability of of full scale, underconditions of constant temperature and pressure. In terms of volume fractions its response to CO2shallnot exce

28、ed as CO. Its response to water vapour shall not exceed as CO.5.5 Ignition device, effecting flameless ignition. Experience has shown that the lighting process can influencethe CO yield considerably. The lighters shall light the cigarettes at the first attempt without either touching orpre-charring

29、the cigarettes. The CO yields are increased by higher lighting intensity.5.6 Barometer, capable of measuring atmospheric pressures to the nearest .5.7 Thermometer, capable of measuring temperature to the nearest .6 Standard gas mixturesMake-up gas shall be nitrogen as other gases can change the dete

30、cted response of carbon monoxide. Gasesused should be of high purity (with low content of carbon dioxide) and used within the manufacturers time limits.The NDIR analyser should be calibrated with at least three standard gas mixtures of accurately knownconcentrations within a relative error of coveri

31、ng the expected range in such a way as to avoid extrapolationof the calibration curve. Typically volume fractions of about , and of CO in nitrogen are appropriate.7 Procedure7.1 ConditioningCondition the test portion taken from and representative of the laboratory sample in accordance with ISO 3402.

32、Verify that equilibrium has been properly attained as described in ISO 3402.The atmosphere in the laboratory where the smoking is to be carried out shall also be in accordance withISO 3402. Place the conditioned test portion in an airtight container (just large enough to contain the portion)and remo

33、ve each cigarette from the container just before smoking.4% 6%2h0,2 %3l10 l0% 10 % 0,5 l/min 5 l/min1% 1% 0,2 %10 %0,05 % 2% 0,05 %0,1 kPa0,1C2%1% 3% 5%6 DIN ISO 8454:2012-02 7.2 Calibration of the NDIR analyser7.2.1 Warm up the instrument according to the manufacturers recommendations, purge the in

34、strument withair and adjust to read zero.7.2.2 Fill a previously evacuated vapour-phase collection container with the standard gas mixture of a volumefraction of about CO, re-evacuate and refill with gas. Ensure that the gas in the container is at ambienttemperature and pressure. Introduce the gas i

35、nto the measuring cell using the system sampling pump allowingto for equilibration of pressure of the analyser. Note the reading on the analyser concentration displaywhen a steady value has been obtained.If necessary, adjust the analyser reading to agree with the certified value of the standard gas.

36、7.2.3 Repeat the procedure as specified in 7.2.2 for at least two other standard gas mixtures. If there is adifference of greater than a volume fraction of CO between the observed and expected values, attentionshould be given to the analyser linearity.7.2.4 Recalibrate the instrument at least once a

37、 week, using the standard gases. The calibration shall be linearwithin the limits reported in 5.4.7.2.5 Check the calibration prior to the measurement using the standard gas containing a volume fraction ofabout carbon monoxide. If there is a difference greater than a volume fraction of CO betweenobs

38、erved and expected values, repeat the full calibration.7.3 Smoking and collection of vapour phase7.3.1 Preparation of vapour-phase collection systemPrepare the system using the instructions pertinent to the equipment fitted.Ensure that the vapour-phase collecting device has been completely flushed w

39、ith ambient air and evacuatedbefore the start of the smoking process. There shall not be any residual vacuum upstream of the collectiondevice before smoking.7.3.2 Smoking procedure7.3.2.1 Smoke the cigarettes in accordance with the procedure stated in ISO 4387.7.3.2.2 For linear smoking machines: af

40、ter completion of smoking each of the first four cigarettes, remove thecigarette butt and take one clearing puff for each trap. After completion of the smoking of all five cigarettes fiveclearing puffs shall be taken.7.3.2.3 For rotary smoking machines: after completion of the smoking run, remove th

41、e cigarette butts and takefive clearing puffs.7.3.2.4 Record the total number of puffs taken on each channel, i.e. smoking puffs plus clearing puffs.7.4 Measurement of carbon monoxide volume concentration7.4.1 Recheck the calibration of the analyser (see 7.2.5) and introduce the vapour phase into th

42、e measuringcell of the analyser under the same conditions of ambient temperature and pressure as for sampling and thesame gas flow rate as used during calibration. Read the analyser display giving the carbon monoxideconcentration. Recalibration may be necessary when the barometric pressure has chang

43、ed for more thanand the CO analyser has no internal compensation.7.4.2 At the end of each smoking, the vapour-phase collection container shall be emptied. The apparatus isthen ready for the next smoking starting at step 7.3.2.1.5%5s 10 s0,2 %5% 0,2 %10 kPa7 DIN ISO 8454:2012-02 8 Expression of resul

44、ts8.1 Calculation of the average volume of carbon monoxide per cigaretteThe average volume of carbon monoxide per cigarette is given by Equation (1):(1)whereis the average volume of carbon monoxide per cigarette, in millilitres;is the percentage by volume of carbon monoxide observed;is the puff volu

45、me, in millilitres;is the number of puffs in the measured sample (including clearing puffs);is the ambient pressure, in kilopascals;is the standard atmospheric pressure, in kilopascals;is the number of cigarettes smoked;is the temperature for the triple point of water, in Kelvin;is the ambient tempe

46、rature, in degrees centigrade.In the calculation the following values can be used:and rounded values of ( ) and ( ).8.2 Calculation of the average mass of carbon monoxide per cigaretteThe average mass of carbon monoxide per cigarette is given by Equation (2):(2)whereis the average mass of carbon mon

47、oxide per cigarette, in milligrams;is the molar mass of carbon monoxide, in grams per mole;is the molar volume of an ideal gas, in litres per mole.In the calculation the following values can be used:Rounded values of ( ) and ( ).9 Repeatability and reproducibilityAn international collaborative study

48、 1 conducted in 2003, involving 58 laboratories and eight samples (sevencommercial brands and the CORESTA monitor test piece CM4), gave the following values for this method.Vas=C V N pT0S 100 p0 (t + T0)VasCVNpp0ST0tV = 35 ml p0101,3 kPa T0273 Kmcig= VasMCOVmmcigMCOVmMCO28 g/mol Vm22,4 l/mol8 DIN ISO 8454:2012-02 The difference between two single results found on matched cigarette samples by the same operator using thesame apparatus within the shortest feasible time interval will exceed the repeatability, , on average not